Triethylamine → HCID 178481869, 화합물

HRID 1247779

반응식

HRID 1247779 반응식
[C:1]([O:5][C:6]([NH:8][C:9]([NH:18][C:19]([O:21][C:22]([CH3:25])([CH3:24])[CH3:23])=[O:20])=[N:10]S(C(F)(F)F)(=O)=O)=[O:7])([CH3:4])([CH3:3])[CH3:2].S(=O)(=O)(O)O.N[C:32]1[CH:33]=[N:34][N:35]([CH3:38])[C:36]=1[NH2:37].C(N(CC)CC)C.C(OCC)(=O)C>ClCCl.O>[NH2:37][C:36]1[N:35]([CH3:38])[N:34]=[CH:33][C:32]=1[NH:10][C:9]([NH:18][C:19]([O:21][C:22]([CH3:25])([CH3:24])[CH3:23])=[O:20])=[N:8][C:6]([O:5][C:1]([CH3:4])([CH3:3])[CH3:2])=[O:7]

참가 물질

7

반응물 4

HCID 8471TriethylamineHCID 8857Ethyl AcetateHCID 36945701,3-Di-Boc-2-(trifluoromethylsulfonyl)guanidineHCID 219045711H-Pyrazole, 4,5-diamine-1-methyl-, sulfate (1:1)

생성물 1

HCID 178481869HCID 178481869, 화합물수율 68.9%

시약·촉매·용매 2

HCID 962Water용매HCID 6344Dichloromethane용매

실험 절차

To a solution of 1,3-bis(tert-butoxycarbonyl)-2-(trifluoromethylsulfonyl)guanidine (22.3 g) in dichloromethane (100 ml) were added 4,5-diamino-1-methylpyrazole sulfuric acid salt (10 g) and triethylamine (33.2 ml) at 4° C., and the mixture was stirred at room temperature overnight. The reaction mixture was poured into a mixture of ethyl acetate and water. The aqueous layer was separated, and the organic layer was washed with brine, dried over anhydrous magnesium sulfate and filtered. The filtrate was concentrated in vacuo. The concentrate was poured into acetonitrile, and the resulting precipitate was collected by filtration and dried in vacuo to give 5-amino-4-[2′,3′-bis(tert-butoxycarbonyl)guanidino]-1-methylpyrazole (11.62 g).

후처리

  1. customThe aqueous layer was separated
  2. washthe organic layer was washed with brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. concentrationThe filtrate was concentrated in vacuo
  6. additionThe concentrate was poured into acetonitrile
  7. filtrationthe resulting precipitate was collected by filtration
  8. customdried in vacuo

출처 및 근거

ORD 기록
ord-2712a3eda6524cefae95afae20296eb2
출처 데이터셋
uspto-grants-2006_10
특허 번호
US07129232B2

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